反应详情

1.0 g of methyl 2-acetyl-6-[(4,6-dimethoxypyrimidin-2-yl)oxy]benzoate, 1.0 g of allyloxyamine hydrochloride and 0.9 g of potassium acetate were added to 30 ml of methanol, and were refluxed with stirring for 5 hours. The reaction mixture was then poured into a cold water, and was extracted with ethyl acetate. The organic layer thus formed was washed with firstly dilute hydrochloric acid, then sodium hydrogencarbonate and water in sequence. The organic layer thus washed was then dried and concentrated. The residue oily product was purified by column chromatography to obtain 0.54 g of the aimed compound (melting point=76° to 78° C.) at a yield of 46% as a colorless transparent crystal.

1. temperaturewere refluxed
2. extractionwas extracted with ethyl acetate
3. customThe organic layer thus formed
4. washwas washed with firstly dilute hydrochloric acid
5. washThe organic layer thus washed
6. customwas then dried
7. concentrationconcentrated
8. customThe residue oily product was purified by column chromatography